Joint Oil Analysis Program Spectrometer Standards SCP Science (Conostan) Qualification Report For D19-0, D3-100, and D12-XXX Series Standards

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1 Joint Oil Analysis Program Spectrometer Standards SCP Science (Conostan) Qualification Report For D19-0, D3-100, and D12-XXX Series Standards NF&LCFT REPORT 441/ Prepared By: MICHAEL PERETICH, PHD Navy Oil Analysis Technical Expert AIR NAVAIR Public Release Distribution Statement A - Approved for public release; distribution is unlimited

2 Page ii Report prepared and released by: Naval Air Systems Command Naval Fuels & Lubricants CFT Elmer Road Patuxent River MD Reviewed and Approved by: PEDRO FARIAS Navy Oil Analysis Program Manager AIR JOHN KRIZOVENSKY Chemistry Laboratory Supervisor AIR JAMES McDONNELL Lubricants Team Lead AIR Released by: DOUGLAS F. MEARNS Fuels & Lubricants Systems Engineer AIR-4.4.1

3 Page iii TABLE OF CONTENTS Page LIST OF TABLES... iv EXECUTIVE SUMMARY... v LIST OF ACRONYMS/ABBREVIATIONS... vi 1.0 BACKGROUND OBJECTIVE APPROACH DISCUSSION CONCLUSIONS RECOMMENDATIONS REFERENCES... 9

4 Page iv LIST OF TABLES Table Title Page Table I. Test Methods... 2 Table II. Candidate Type D19-0 Physical Property Results Table III. Candidate Type D19-0 Rotrode-AES Results... 4 Table IV. Candidate Type D19-0 ICP-AES Results... 4 Table V. Candidate Type D12-XXX Physical Property Results... 5 Table VI. Candidate Type D12-XXX Rotrode-AES Results... 6 Table VII. Retest of Candidate Type D12-XXX Rotrode-AES Results... 6 Table VIII. Candidate Type D12-XXX ICP-AES Results... 6 Table IX. Candidate Type D3-100 Physical Properties, Rotrode AES and ICP AES Results... 7

5 Page v EXECUTIVE SUMMARY The Joint Oil Analysis Program previously revised the specification for their spectrometric oil standards in order to incorporate an ICP-AES test method and to transition to commercially manufactured spectrometric oil standards. Historically, a Rotrode-AES test method was the only elemental test method used to verify the quality of the spectrometric oil standards. The Rotrode-AES test method was a labor and time intensive process that did not exhibit a high level of accuracy and repeatability. The JOAP wanted to incorporate an ICP- AES test method in order to obtain a more accurate determination of the true concentration of the elements in the spectrometric oil standards and to reduce the cost and time needed to conduct quality assurance. Both the Rotrode-AES and ICP-AES test methods are now part of the qualification inspection in order to ensure that commercially manufactured spectrometric oil standards are identical to those that have been produced in-house by the JOAP. This report covers the qualification testing of Type D19-0, Type D12-XXX series, and Type D3-100, candidate spectrometric oil standards submitted by SCP Science (Conostan) against the requirements of MIL-DTL In general, the candidate spectrometric oil standards met the requirements of the specification. A few specific data points were analyzed and waived based on alternative testing and analysis. As a result of this testing and analysis effort the SCP Science (Conostan) Type D19-0, Type D12-XXX series, and Type D3-100 spectrometric oil standards have been qualified to the specification. Since this qualification testing effort was only the second time the full range of data required by MIL-DTL has been collected, analysis of the data has led to the conclusion that several of the requirements of the specification need revision. Several changes to the specification are therefore under consideration based on historical knowledge of JOAP manufactured spectrometric oil standards and the MIL-DTL qualification data and analysis from all of the commercially manufactured spectrometric oil standards.

6 Page vi LIST OF ACRONYMS/ABBREVIATIONS Joint Oil Analysis Program... JOAP Joint Oil Analysis Program-Executive Committee...JOAP-EC Rotrode Atomic Emission Spectroscopy... Rotrode-AES Inductively Coupled Plasma Atomic Emission Spectroscopy... ICP-AES

7 Page 1 Joint Oil Analysis Program Spectrometer Standards SCP Science (Conostan) Qualification Report For D19-0, D3-100, and D12-XXX Series Standards 1.0 BACKGROUND The Joint Oil Analysis Program, reference (a), previously revised the specification for their spectrometric oil standards in order to incorporate an ICP-AES test method and to transition to commercially manufactured spectrometric oil standards. Historically a Rotrode-AES test method was the only elemental test method used to verify the quality of the spectrometric oil standards. The Rotrode-AES test method was a labor and time intensive process that did not exhibit a high level of accuracy and repeatability. The JOAP wanted to incorporate an ICP-AES test method in order to obtain a more accurate determination of the true concentration of the elements in the spectrometric oil standards and to reduce the cost and time needed to conduct quality assurance. Both the Rotrode-AES and ICP-AES test methods are now part of the qualification inspection in order to ensure that commercially manufactured spectrometric oil standards are identical to those that have been produced in-house by the JOAP. SCP Science (Conostan) submitted Type D19-0, Type D12-XXX series, and Type D3-100 spectrometric oil standards that were manufactured to meet the requirements of MIL-DTL Testing was accomplished at the NAVAIR Patuxent River MD test facility in accordance with the latest revision of MIL-DTL-85694, reference (b). 2.0 OBJECTIVE The objective of this testing is to qualify a second commercial vendor, SCP Science (Conostan), for the production of blended spectrometric oil standards that are used in calibrating and verifying the calibration of spectrometers used in spectrometric analysis of metallic elements found in oils and other fluids. 3.0 APPROACH The test methods for qualification inspection are specified in Table I. The density, viscosity, viscosity index, trace sediment, pour point, and flash point test methods were conducted in accordance with the corresponding ASTM test method listed in Table I.

8 Page 2 TABLE I. Test Methods Physical property Test Method Density at 60 F ASTM D4052 Viscosity (mm 2 /s at 100 C) ASTM D445 Viscosity Index, Min ASTM D2270 Trace Sediment ASTM D2273 Pour point ASTM D97 Flash point, minimum (COC) ASTM D92 Metal Elements (Rotrode-AES) ASTM D6595 Metal Elements (ICP-AES) ASTM D5185 The Rotrode-AES test method was conducted in accordance with ASTM D6595. Testing of candidate spectrometric oil standards was done as a statistical analysis and performed on the data generated by the spectrometric analysis to provide an accuracy index and repeatability index for each element involved. The results were obtained with a JOAP-EC approved Spectroil M/N spectrometer (S/N 6403). The testing consisted of ten replicates of each candidate spectrometric standard. The ICP-AES test method was conducted in accordance with ASTM D5185. Testing of spectrometric oil standards was done as a statistical analysis and performed on the data generated by the spectrometric analysis to provide an accuracy index for each element involved. The results were obtained with a JOAP-EC approved ICP spectrometer (Agilent 725 Series ICP-OES spectrometer). The ICP spectrometer was calibrated from 0 ppm to 20 ppm using a commercial ICP multi-element spectrometric standard. Candidate spectrometric oil standards were diluted on a weight-by-weight basis with a suitable ICP solvent. Candidate spectrometric oil standards in concentrations 5 ppm, 10 ppm, 30 ppm, and 50 ppm were diluted tenfold while candidate standards in concentrations 80 ppm, 100 ppm, 120 ppm, 300 ppm, 500 ppm, 700 ppm, and 900 ppm were diluted to 5 ppm. The testing consisted of five replicates of each candidate spectrometric standard. 4.0 DISCUSSION This section details the analysis of the data in accordance with MIL-DTL qualification testing. In the situations where a requirement was not met, the NOAP-EC reviewed the data and determined if the specific requirement can be waived due to factors that influenced some chemical and physical properties that were not taken into consideration during the initial development of the specification.

9 Page Type D19-0 The Type D19-0 spectrometric oil standard submitted by the candidate met the requirements for density at 60 F, viscosity at 100 C, viscosity index, trace sediment, and flash point (Table II). TABLE II. Candidate Type D19-0 Physical Property Results TEST METHOD UNITS SAMPLES D19-0 Density at 60 F ASTM D4052 kg/l Viscosity at 100 C ASTM D445 cst 40 C ASTM D445 cst Viscosity Index ASTM D2270 No Units 96 Pour Point ASTM D97 C Flash Point ASTM D92 C Water & Sediment ASTM D2273 % NOTE: Red numbers indicate the requirement not being met The D19-0 did not meet the requirement for Pour Point however the measured value is within the reproducibility for ASTM D97 and the NOAP-EC is willing to waive the requirement. The Type D19-0 spectrometric oil standard submitted by the candidate met the requirement for Rotrode-AES (Table III) and ICP-AES (Table IV).

10 Page 4 TABLE III. Candidate Type D19-0 Rotrode-AES Results TEST METHOD UNITS SAMPLES D19-0 Trace Metal: ASTM D6595 ppm Mean Stdev Al Cr Cu Fe Pb Mg Ni Si Ag Na Sn Ti B Mo Zn Ba Cd Mn V TABLE IV. Candidate Type D19-0 ICP AES Results TEST METHOD UNITS SAMPLES D19-0 ICP ASTM D5185 ppm Al Cr Cu Fe Pb Mg Ni Si Ag Na Sn Ti B Mo Zn Ba Cd Mn V Mean The Type D19-0 spectrometric oil standard submitted by the candidate satisfactorily passed the qualification inspection.

11 Page Type D12-XXX Series All of the Type D12-XXX spectrometric oil standards submitted by the candidate met the requirements for density at 60 F, viscosity at 100 C, viscosity index, and trace sediment (Table V). TABLE V. Candidate Type D12-XXX Physical Property Results TEST METHOD UNITS SAMPLES D12-5 D12-10 D12-30 D12-50 D D Density at 60 F ASTM D4052 kg/l Viscosity at 100 C ASTM D445 cst C ASTM D445 cst Viscosity Index ASTM D2270 No Units Pour Point ASTM D97 C Flash Point ASTM D92 C Water & Sediment ASTM D2273 % NOTE: Red numbers indicate the requirement not being met The D12-30 and D12-50 spectrometric oil standards met the physical property requirements while the D12-5, D12-10, and D oil standards met all of the physical property requirements except for flash point and the D oil standard met all of the physical property requirements except for pour point. The D did not meet the requirement for Pour Point; however the measured value is within the reproducibility for ASTM D97 and the NOAP-EC is willing to waive the requirement. The D12-5 and D12-10 did not meet the requirement for Flash Point; however the measured value is within the reproducibility for ASTM D92 and the NOAP-EC is willing to waive the requirement. The high concentration of the metallo-organic concentrates in D has an effect on the flash point which resulted in the requirement for flash point not being met. The significance of the effect was not taken into consideration during the development of the original specification requirements therefore the flash point requirement for D will require revision. At this time the NOAP-EC is waiving the flash point requirement for D All of the Type D12-XXX spectrometric oil standards with the exception of D met the requirement for Rotrode-AES (Table VI). The Rotrode-AES chromium, iron, and nickel accuracies for D were identified as being outside of the Rotrode-AES requirement. Following standard JOAP quality assurance procedure, the D was diluted to 50 ppm using D19-0 and retested to address the accuracy issue. Upon retesting, the Rotrode-AES accuracy and repeatability requirements for all elements were met (Table VII). All of the Type D12-XXX spectrometric oil standards met the requirement for ICP-AES (Table VIII).

12 Page 6 TEST METHOD UNITS TABLE VI. Candidate Type D12-XXX Rotrode-AES Results SAMPLES D12-5 D12-10 D12-30 D12-50 D D Trace Metal: ASTM D6595 ppm Mean Stdev Mean Stdev Mean Stdev Mean Stdev Mean Stdev Mean Stdev Al Cr Cu Fe Pb Mg Ni Si Ag Na Sn Ti NOTE: Red numbers indicate the requirement not being met TABLE VII. Retest of Candidate Type D12-XXX Rotrode-AES Results TEST METHOD UNITS SAMPLES D12-5 D12-10 D12-30 D12-50 D D Trace Metal: ASTM D6595 ppm Mean Stdev Mean Stdev Mean Stdev Mean Stdev Mean Stdev Mean Stdev Al Cr Cu Fe Pb Mg Ni Si Ag Na Sn Ti TEST METHOD UNITS TABLE VIII. Candidate Type D12-XXX ICP-AES Results SAMPLES D12-5 D12-10 D12-30 D12-50 D D ICP ASTM D5185 ppm Al Cr Cu Fe Pb Mg Ni Si Ag Na Sn Ti Mean Mean Mean Mean Mean Mean The Type D12-XXX spectrometric oil standards submitted by the candidate satisfactorily passed the qualification inspection.

13 Page Type D3-100 The Type D3-100 spectrometric oil standard submitted by the candidate met the requirements for density at 60 F, viscosity at 100 C, viscosity index, trace sediment, pour point, Rotrode-AES, and ICP-AES (Table IX). TABLE IX. Candidate Type D3-100 Physical Property, Rotrode AES and ICP AES Results TEST METHOD UNITS SAMPLE D3-100 Density at 60 F ASTM D4052 kg/l Viscosity at 100 C ASTM D445 cst 40 C ASTM D445 cst Viscosity Index ASTM D2270 No Units 93 Pour Point ASTM D97 C Flash Point ASTM D92 C Water & Sediment ASTM D2273 % Trace Metal: ASTM D6595 ppm Mean Stdev B Mo Zn ICP ASTM D5185 ppm Mean B Mo Zn NOTE: Red numbers indicate the requirement not being met The D3-100 did not meet the requirement for Flash Point and is not within the reproducibility for ASTM D92; however the NOAP-EC is willing to waive the requirement due to the fact that current JOAP spectrometric standards have flash points as low as 110 C. The Type D3-100 spectrometric oil standard submitted by the candidate satisfactorily passed the qualification inspection.

14 Page CONCLUSIONS The following spectrometric oil standards submitted by SCP Science (Conostan) have satisfactorily passed the qualification inspection and should be added to the qualified products list for MIL-DTL-85694: Type D19-0 Type D12-XXX (D12-5, D12-10, D12-30, D12-50, D12-100, D12-300) Type D RECOMMENDATIONS A number of issues associated with the specification requirements were brought to light as a result of all of the qualification testing. Several changes to the specification are therefore under consideration. Commercial manufacturers have notified the NOAP-EC that they are having difficulty obtaining SAE J1966, reference (c), oil due to low market demand. The NOAP-EC and commercial manufacturers have been informed that SAE J1899, reference (d) could be an acceptable alternative to SAE J1966 as long as the oil is silicon free however manufacturers are having difficulty obtaining silicon free J1899 for the same reason. Changes to MIL-DTL are therefore under consideration in order to better define chemical and physical property requirements and help address the challenges associated with supply. Density and viscosity are the key physical properties that could have significant influence on Rotrode measurements. Flash point can be most influenced by the metallo-organic concentrates and stabilizer. The base oil has less of an effect on flash point. Current MIL-DTL JOAP spectrometric oil standards have flash points as low as 100 C therefore flash point is a less critical physical property requirement. The pour point test method has a large reproducibility range. In addition, pour point is influenced by the chemical composition of the oil. The challenges that commercial manufacturers are having associated with supply due to market demand could explain a variation in the chemical composition of the oil and thus the higher pour point. Pour point did not appear to adversely influence Rotrode-AES measurements and therefore is a less critical physical property requirement. The NAVAIR Patuxent River MD test facility has recently expanded its test capability by adding instrumentation able to conduct viscosity measurements in accordance with ASTM D7042. For this reason, ASTM D7042 is under consideration for inclusion in the next revision of MIL-DTL , reference (b).

15 Page REFERENCES a. OPNAVINST , Joint Oil Analysis Program, 26 March 2014 b. MIL-DTL-85694A, Detail Specification, Spectrometric Oil Standards, 12 August 2013 c. SAE J1966, Lubricating Oil, Aircraft Piston Engine (non-dispersant Mineral Oil), REV. JUL2005 d. SAE J1899, Lubricating Oil, Aircraft Piston Engine (Ashless-Dispersant), REV. AUG2005

16 Page 10 This Page Intentionally Left Blank

17 Appendix A Page A-1 Appendix A Viscosity Test Data The NAVAIR Patuxent River MD test facility has recently expanded its test capability by adding instrumentation able to conduct viscosity measurements in accordance with ASTM D7042. Viscosity data collected in accordance with ASTM D7042 are presented in Table X in addition to the corresponding viscosity index data. TABLE X. ASTM D7042 Viscosity Results and Corresponding ASTM D2270 Viscosity Index Results TEST METHOD UNITS SAMPLES D19-0 D12-5 D12-10 D12-30 D12-50 D D D3-100 Viscosity at 100 C ASTM D7042 cst C ASTM D7042 cst Viscosity Index ASTM D2270 No Units

18 REPORT DOCUMENTATION PAGE Form Approved OMB No Public reporting burden for this collection of information is estimated to average 1 hour per response, including the time for reviewing instructions, searching existing data sources, gathering and maintaining the data needed, and completing and reviewing this collection of information. Send comments regarding this burden estimate or any other aspect of this collection of information, including suggestions for reducing this burden to Department of Defense, Washington Headquarters Services, Directorate for Information Operations and Reports ( ), 1215 Jefferson Davis Highway, Suite 1204, Arlington, VA Respondents should be aware that notwithstanding any other provision of law, no person shall be subject to any penalty for failing to comply with a collection of information if it does not display a currently valid OMB control number. PLEASE DO NOT RETURN YOUR FORM TO THE ABOVE ADDRESS. 1. REPORT DATE (DD-MM-YYYY) 2. REPORT TYPE Technical 4. TITLE AND SUBTITLE Joint Oil Analysis Program Spectrometer Standards; SCP Science (Conostan) Qualification Report for D19-0, D3-100, and D12-XXX Series Standards 6. AUTHOR(S) Peretich, Michael; Author Farias, Pedro ; Editor Mearns, Douglas ; Editor 3. DATES COVERED (From - To) to a. CONTRACT NUMBER N/A 5b. GRANT NUMBER N/A 5c. PROGRAM ELEMENT NUMBER N/A 5d. PROJECT NUMBER N/A 5e. TASK NUMBER N/A 5f. WORK UNIT NUMBER N/A 7. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES) 8. PERFORMING ORGANIZATION REPORT NUMBER Naval Fuels & Lubricants Cross NF&LCFT Report 441/ Functional Team Elmer Road Patuxent River, MD SPONSORING / MONITORING AGENCY NAME(S) AND ADDRESS(ES) 10. SPONSOR/MONITOR S ACRONYM(S) Naval Air Systems Command N/A NPRE Program Cedar Point Road 11. SPONSOR/MONITOR S REPORT Patuxent River MD NUMBER(S) N/A 12. DISTRIBUTION / AVAILABILITY STATEMENT A Approved for public release; distribution is unlimited. 13. SUPPLEMENTARY NOTES N/A 14. ABSTRACT The Joint Oil Analysis Program previously revised the specification for their spectrometric oil standards in order to incorporate an ICP-AES test method and to transition to commercially manufactured spectrometric oil standards. Historically, a Rotrode-AES test method was the only elemental test method used to verify the quality of the spectrometric oil standards. The Rotrode-AES test method was a labor and time intensive process that did not exhibit a high level of accuracy and repeatability. The JOAP wanted to incorporate an ICP-AES test method in order to obtain a more accurate determination of the true concentration of the elements in the spectrometric oil standards and to reduce the cost and time needed to conduct quality assurance. Both the Rotrode-AES and ICP-AES test methods are now part of the qualification inspection in order to ensure that commercially manufactured spectrometric oil standards are identical to those that have been produced in-house by the JOAP. This report covers the qualification testing of Type D19-0, Type D12-XXX series, and Type D3-100, candidate spectrometric oil standards submitted by SCP Science (Conostan) against the requirements of MIL-DTL In general, the candidate spectrometric oil standards met the requirements of the specification. A few specific data points were analyzed and waived based on alternative testing and analysis. As a result of this testing and analysis effort the SCP Science (Conostan) Type D19-0, Type D12-XXX series, and Type D3-100 spectrometric oil standards have been qualified to the specification. Since this qualification testing effort was only the second time the full range of data required by MIL-DTL has been collected, analysis of the data has led to the conclusion that several of the requirements of the specification need revision. Several changes to the specification are therefore under consideration based on historical knowledge of JOAP manufactured spectrometric oil standards and the MIL-DTL qualification data and analysis from all of the commercially manufactured spectrometric oil standards. 15. SUBJECT TERMS Joint Oil Analysis Program, Spectrometer Standards 16. SECURITY CLASSIFICATION OF: 17. LIMITATION OF ABSTRACT a. REPORT UNCLASSIFIED b. ABSTRACT UNCLASSIFIED c. THIS PAGE UNCLASSIFIED Unclassified Unlimited 18. NUMBER OF PAGES 19a. NAME OF RESPONSIBLE PERSON Douglas F. Mearns 18 19b. TELEPHONE NUMBER (include area code) Standard Form 298 (Rev. 8-98) Prescribed by ANSI Std. Z39.18

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